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Rezumat GPC

The molecular weight of the PDMS was measured using gel permeation
chromatography (GPC) in toluene with PDMS standards (American Polymer
Standards, Scientific Polymer Products) while PS/PDMS blends were measured in
tetrahydrofuran (THF) with PS standards (Polymer Laboratories).
A Waters 150C GPC was used at 25C with three Phenogel columns (porosities of
500 , 1000 , and 10,000 ). Differential refractive index and ultra-violet (UV)
detectors were used.
For amine-containing polymers, phenyl isocyanate was added to quench any
remaining free amine and to prevent adsorption of the amine groups onto the GPC
Functionality of homopolymers was determined using nuclear magnetic resonance
(NMR), infra-red spectroscopy (IR), thin layer chromatography (TLC) and solution
coupling with GPC (25). For the melt blends, the areas of the GPC peaks were
calculated by Gaussian fits to the GPC chromatograms using Microcal Origin 5.0
software (14). For the PS/PDMS blends, the ratio of the peak area corresponding to
block copolymer product to the total area of the homopolymer and block copolymer
gives the conversion based on PS. Since PDMS is isorefractive with THF and invisible
in the UV range of the PS, the conversion was based on PS. The conversion of the
limiting reagent (the functional group attached to the PDMS) was determined given
the PS conversion, the molecular weights, functionality and mass of the PS and
PDMS. Homopolymer viscosities were measured with a Rheometrics Dynamic Stress
Rheometer (DSR) using a parallel plate geometry in the oscillatory mode for the PA6
at 235C or PS at 200C. The strain was kept below 10% to keep the experiment in
the linear viscoelastic regime. The PDMS liquids were measured in steady-shear
mode with a parallel plate geometry at 200C. All the PDMS samples used here
were Newtonian. Mixing. Melt blending was performed at 200C for the PS/PDMS
blends and 235C for the PA6/PDMS blends using a cup and rotor mixer at 330 rpm.
(MiniMAX, Custom Scientific Products, cup diameter 13 mm). PA6 was dried for
several hours at 100C under vacuum to remove moisture. A nitrogen blanket was
used to minimize polymer degradation. For the PS/PDMS blends, three steel balls
each having a diameter of 3.8 mm were placed inside the cup to improve the mixing
(26, 27). Typical batch sizes for the MiniMAX were about 0.3 g. Samples for kinetic
analysis were 510 mg while morphology samples were typically 20 mg. All
heterogenous blends were 80 wt% PS or PA6 with the exception of PA6/D38-r-An
which was 70 wt% PA6. PA6/PDMS blends were also compounded using a 16 mm
diameter co-rotating twin-screw extruder (PRISM, Welding Engineers). The length to
diameter ratio was 25:1 and a screw rotation rate of 50 rpm was used. The PA6 was
fed through the main auger feeder at a rate of 0.46 kg/h. PDMS was fed into the

extruder into a downstream port from a syringe pump at 0.12 kg/h. The molten
blend passed through a 24 mm exit section with a 1 mm diameter die plate and the
resulting strand was cooled in a water bath, dried and pelletized. Static annealing of
PS/PDMS blends to evaluate stability was done by sealing blend samples under
vacuum at a pressure of 110 mTorr in glass ampoules. The ampoules were then
placed in an oil bath at 200C for 30 minutes. The blends were termed stable if the
dispersed phase particle size measured from electron micrographs did not increase
by more than 20% after annealing.